The synthesis of novel fluorous vic-dioxime derivitives and their metal complexes, the determination of their solubility in a scco2 medium and their use as precursors in deposition

Vic-dioxime derivative metal complexes were synthesized in order to determine their solubility in a scCO2 medium and their use as precursors in the deposition of metal nanoparticles. Their structures were determined and their use in deposition onto silicagel and ?-alumina in scCO2 was tested in this study. Pd(II) and Cu(II) metal complexes with vic-dioxime ligands and were synthesized for this purpose. The ligands were made by reacting various aniline derivatives with anti-monochloro glyoxime. In order to increase the solubility of the complexes in scCO2, some of the ligands were synthesized from aniline derivatives with long fluorous chains. All ligands and complexes were synthesized and characterized via various analyses including FT-IR, 1H, 19F NMR, UV-Vis and magnetic susceptibility. The solubility of the metal complexes in supercritical medium was also determined. The synthesized metal complexes were used as precursors for the deposition of the metals on solid supports in a scCO2 medium resulting in the synthesis of nano-sized metal catalysts. The size of the synthesized nanocatalysts was analyzed by TEM and XRD. The Pd particles ranged from 2-16nm and the Cu nanoparticles ranged from 3-20nm. The activity of these catalysts in a hydrogenation reaction of olefins was analyzed using GC.